Assessment of mefenamic acid polymorphs in commercial tablets using chemometric coupled to MIR and NIR spectroscopies. Prediction of dissolution performance

Antonio, Marina; Maggio, Rubén M.

doi:10.1016/j.jpba.2017.11.053

Cited by 24 publications

(11 citation statements)

References 25 publications

(22 reference statements)

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“…Form II showed only one endothermic peak corresponding to its melting point at 233 ºC. The results obtained were in agree with literature [19,27].…”

Section: Characterization Of Mfa Pure Polymorphs and Commercial Formsupporting

confidence: 92%

“…The polymorphs of MFA (Form I and Form II) were obtained as previously reported [19] and unequivocally characterized by optical microscopy (Figure S1), MIR and NIR spectroscopy Figure S2), melting point determination and DSC. The obtained results were in full agreement with the literature [24,25,26].…”

Section: Characterization Of Mfa Pure Polymorphs and Commercial Formmentioning

confidence: 84%

“…There, PCA allow data compression and visualization, and further statistical analysis using Mahalanobis distance [17,18]. Additionally, NIR spectroscopy was the only vibrational spectroscopy able to successfully predict polymorphic content in commercial tablets of Mefenamic acid, using the obtained polymorphic content to predict the solubility performance [19].…”

Section: A C C E P T E Dmentioning

confidence: 99%

“…MFA pure forms (Form I and Form II) used as references were prepared according to recently reported procedures [19]. Identity of purity of the forms were confirmed by optical microscopy, MIR and NIR spectroscopy, melting point determination and DSC.…”

Section: Mfa Pure Formsmentioning

confidence: 99%

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Chemometric study of the excipients’ influence on polymorphic-behavior. Mefenamic acid as case of study

Antonio

Calvo

Maggio

2019

Journal of Pharmaceutical and Biomedical Analysis

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The assessment of polymorphism is a problematical issue for regulatory agencies, because variations among crystalline forms of active pharmaceutical ingredient (API) can lead to changes in the efficacy and safety of formulated product. Such conversions are very hard to be detected, thus, the development of techniques for the identification, characterization and quantification of polymorphs results essential in all stages of the manufacturing process. The presence of excipients in formulated products may change the crystal stability of an API, by catalyzing a polymorphic transformation or stabilizing the less stable form. As paradox, all suitable analytical techniques (spectroscopies, thermal analysis, NMR and DRX, and others) for polymorphic analysis are affected by excipients. A deep understanding of the polymorphism-excipient relationship is in full accordance with Quality by Design (QbD) paradigm, the systematic approach focused in quality building into a product based in the full understanding of the products and process. In this work, a novel approach based on thermal stress, MIR monitoring, multivariate curve resolution with alternating least squares (MCR-ALS) and kinetic analysis was developed and applied to monitor polymorphism behavior of model API in formulated products. Commercial tablets, physical mixtures and commercial API, were processed and analyzed under the proposed approach. Commercial tablets of MFA revealed a fast conversion to Form II, contrasting to the behavior of the pure API. Physical mixtures showed similar behavior to commercial tablets, thus reduction in transformation times was related to MFA-excipients physical interaction, even at surface level. Calorimetric studies support the conclusion obtained. The developed approach could be extended to others APIs and other stress sources (humidity, solvents, mechanical forces and its combinations), being a valuable tool for QbD environment.

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“…Form II showed only one endothermic peak corresponding to its melting point at 233 ºC. The results obtained were in agree with literature [19,27].…”

Section: Characterization Of Mfa Pure Polymorphs and Commercial Formsupporting

confidence: 92%

Section: Characterization Of Mfa Pure Polymorphs and Commercial Formmentioning

confidence: 84%

Section: A C C E P T E Dmentioning

confidence: 99%

Section: Mfa Pure Formsmentioning

confidence: 99%

See 2 more Smart Citations

Chemometric study of the excipients’ influence on polymorphic-behavior. Mefenamic acid as case of study

Antonio

Calvo

Maggio

2019

Journal of Pharmaceutical and Biomedical Analysis

Self Cite

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show abstract

“…I n t hei r st udy , i t was shown t hat t he NI RS model was abl e t o pr edi ct di ssol ut i on of i ndi vi dual t abl et based on NI R spect r um i n a cont i nuous manuf act ur i ng syst em. Anot her r R ec ent example of utilizing NIR was presented by Antonio and Maggio (2018) who linked polymorphic form I content of mefenamic acid with dissolution and thus showed that a NIR-PLS model may act as a val i d t ool t o est i mat e di ssol ut i on prof i l es of a commer ci al t abl et . Speci f i c met hodol ogy t o pr edi ct API di ssol ut i on based on di si nt egr ant chemi cal i nf or mat i on obt ai ned wi t h NI R chemi cal i magi ng i s descr i bed i n t he wor k of Yekpe et al .…”

Section: Introductionmentioning

confidence: 99%